Process of imparting alpha green fluorescence to lubricating oil



Patented Jan. 2 6, 1932 Jenn c. annex, or nos anc ents, vvrnr n. man, or nosnncnnns COUNTY, am) Joni: n'nrccoimnnn, or wnrrrrnn, cnrirrorarm, assrenclne, an arnsun nssiomnnrs, ro nrcnrrnnn ornoonrnna' or oaarroanra, or nos anenrins, oanmoimm, a con- :eonarron or neither rnocnss or manna a c lio Drawing.

a solvent, and then utilizing the solvent con- 1o Wirt D. Rial and John R. McConnell, Serial taining the extracted green fluorescent bodies for improving the quality or imparting a desired green fluorescence to a lubricating oil stock. This application is a continuation in part of the application of John G, Black,

No. 141,424 filed October 13, 1926, process of imparting fluorescence to oil.

As stated in that pending application, the trade associates a green fluorescent lubricating oil stock with quality, therefore it is desired for commercial reasons to im art a green fluorescence to certain grades 0 lubricatin oil stock.

It 1s generally known to'thoseskilled in the art,'that certain lubricating oil stocks without this green fluorescence may contain an undesirable fluorescence and that this 1111-. desirable fluorescence usually is characteristic of a stock which has been derived by distillation of any crude petroleum oil.

In the manufacture of lubricatin oil from crude petroleum oil free from aspha t, or substantially free from asphalt, a green fluorescence will result in the residuum remaining after the removal of the lower boiling oils, even though the residuum has been sub ected to a light cracking operation to crystallize the amorphous wax contained therein, and a lubricating oil stock-can be produced from the same with a green fluorescence. Also a lubricating oil with a green fluorescence can be made by acid treating an asphalt base oil residuum 1f suflicient acid is employed to remove substantially all the asphaltic content. However, such methods are impracticable since very lar e amounts of acid must be used, thus entailing low yields of the finished lubricating oil. a g

It is an object of this invention to extract green fluorescent bodies from a coal tar, coal tar pitch or distillates of-the same with a solvent and then utilize the solvent containing the extracted green fluorescent bodies tor improving the quality or imparting a desired green fluorescence to lubricating oil stocks,

Application filed an is,

tar distillates, or coal tar. pitch with 1927. terlal tic. 3%,1'58.

viewed by reflected light, but will be generally characterized by a green fluorescence, and will be further characterized b reddish brown, yellow, or shades 0 yellow when viewed by transmitted light.

We have found that certain bodies extracted from coal tar coal tar pitch, or distillates of the same, wil impart to a lubricating oil stock a green fluorescence.

The process of this application consists in concentrating these green fluorescent bodies in a solvent or medium, and then commingling the concentrated extract with a lubricating oil stock in quantities suflicient to produce the desired green fluorescence. It is an important advantage of this process that by-employing a concentrated fluorescent extract, substantially no impurities associated with the fluorescence material are introduced into the oil,

As an exam is of suitable materials from which green uorescent bodies may be extracted for imparting a desired green fluorescence to a lubricating) oil stoc coal tar pitch, or high oiling distillates oi the same may be used. A coal tar pitch which does not contain low boilin hydrocarbons is preferred, although coa tar or coal tar pitch containingsmall percentages of low boilin hydrocarbons. may be employed, and t a low boiling hydrocarbons eliminated by, distillation, preferably after the extraction process and before the addi-' tion to the lubricating oil stock. However,

it is to be understood that this elimination a red,

coal tar of the low boiling hydrocarbons, if any is contained therein, may be carried out after the additidn of the fluorescent extractto the lubricating'oil stock by a subsequent distillate tion or reduction operation.

The solvent or medium to be employed for let;

the solvent, preferably near the boiling point of the solvent. The extract in the required proportions is added to the lubricatin oil stock and the solvent removed by vo atilization. I

We have found it more desirable, however, to employ high boiling hydrocarbon oils such for example, as a lubricating oil havin a flash point the same or higher than the lu ricatin oil stock to-which the fluorescent extract is to be added. The solvent or medium, preferably lubricating oil stock, is commingled with approximately 1 to approximately per cent y weight of coal tar pitch or other high flash coal tar residues which contain extractable green fluorescent bodies,.

at a temperature of ap roximately 230 to 300 degrees F., and pre erably in the presence of a decolorizing clay which will absorb all the undesired constituents of the petroleum oil pitch, and also act as a filter medium to prevent any finely comminuted particles from passing through with the solvent or medium. In case a decolorizin clay is not em loyed in the manufacture o the extract, which is used for imparting a desired green fluorescence to the lubricating oil stock, it may be added directly to the lubricating 011 stock to which the fluorescent bodies are to be added, and thereafter clarified and decolorized to the desired degree by methods well known in the art.

In case a volatile solvent or medium is employed, approximately the same amount of coal tar itch, coal tar, or coal tar distillate, that is, fiiom 1 to as high as 25 per cent by weight, or hi her, is employed at a temperature preferably near the boiling point of the solvent or medium, although normal temperatures may be employed with such solvents as benzol or gasoline. After the petroleum pitch has been commingled at the required temperature with the solvent or medium, which may or may not have been fil-' tered in the presence of a decolorizing clay, this concentrated extract is then added in the required amount to the lubricating oil stock, to which the desired fluorescence is to be imparted, and the volatile solvent separated by a distillation operation, or the lubricating oil stock commingled with the concentrated fluorescent extract may be first clarified and decolorized by means of a decolorizing agent, and the volatile solvent thereafter separated by distillation. In case a coal tar distillate is employed that fraction known as middle oil is preferably used, and preferably having boiling points ranging from approximately 400 to 600 de rees F.

As a specific example 0 obtaining a green fluorescent extract from coal tar pitch suitable for imparting a green fluorescence to lubricating oil, a coal tar pitch havin a penetration of approximately 2 was dissolvcd in benzol, approximately at the rate of 25 parts of oil pitch to 75 parts of benzol. This mixture was then treated with sulfuric acid in uantities suflicient to precipitate substantial 1;; all the asphaltic material contained t erein. After the removal of the precipitated asphalt and products of the acid reaction, a green fluorescent extract was ob tained in a benzol solution. After removal of the benzol by distillation there was produced a concentrated green fluorescent ex tract suitable for producing the desired green fluorescence when added to a lubricating oil stock. In like manner a lubricating oil stock ma be used as the solvent instead of benzol.

n the preferred method of operating this invention, the lubricating oil stock is preferably acid treated before the addition of the concentrated green fluorescent extract, after which the sludge is removed, and the acid treated oil is then commingled with the required amountof concentrated green fluorescent extract, which is also preferably an acid treated lubricatin oil stock containing a high percentage 0% green fluorescent bodies made in the manner heretofore described. The commingled lubricating oil stock containing the green fluorescent extract is then clarified and decolorized by well-known methods.

By the term solvent or medium, we mean an oil which will dissolve or retain in a colloidal suspension the reen fluorescent bodies from a coal tar pitc While the process herein described is Well adapted for carrying out the objects of the present invention, it is to be understood that various modifications and changes ma be made without de arting from the spirit of the invention anti the invention includes all such changes and modifications as appear in the scope of the appended claims.

We claim: 1. A process of simultaneous refining and nnparting a desired green fluorescence to a lubricating oil which is lacking in the same, comprisin commingling a lubricating oil with a hy rocarbon oil containing green fluorescent bodies extracted from a coal tar rcsiduum.

2. A process of simultaneous refining and imparting a desired green fluorescence to lubricating oil which is lacking in the same, comprisln commingling a lubricating oil with a hydrocarbon oil containing green fiuorescent bodies extracted from a coal tar pitch, and then separating the hydrocarbon oil from the lubricating oil and green fluorescent bodies.

3. A process of simultaneous refining and imparting a desired green fluorescence to lubricating oil which is lacking in the same, comprising commingling a lubricating oil with a hydrocarbon oil containing green flu orescent bodies extracted from a coal tar pitch, and then separating the hydrocarbon oil from the lubricating oil and green flu- I ill) bodies with a lubricating oil.

orescent bodies, by distillation) 4. A process of simultaneous refining and imparting a desired green fluorescence to lu-f bricating oil, which is lacking in the same, comprislng bodies from a coal'tar pitch with a hydrocarbon oil, commingling the same with a lubri eating oil and a decolorizing clay at temperatures sufficient to clarify and decolorize the lubricating oil and hydrocarbon oil containing the green fluorescent bodies, and then separating the clarified and decolorized lhbricating oil containing the hydrocarbon oil and green fluorescent bodies from the decolorizing clay and adsorbed constitutents.

a 5. A process for the manufacture of lubricating oil with a desired green fluorescence, comprising dissolving a coal tar pitch con tainlng green fluorescent bodies in a solvent having a boiling point range substantially less than the lubricating oil, treating the extracting green fluorescent solutioncontaining the dissolved coal tar pitch with sulfuric acid in quantities suffi-' cinet to combine with substantially .all of the carbonaceous content; separatiiig the solvent containing the green fluorescent bodies from the acid reaction products; separating by distillation the solvent from the green fluorescent bodies'and finally commingling the concentrated'green fluorescent extract with a lubricating oil.

6. A process for the manufacture of lubri eating oil with a desired green fluorescence, comprising dissolving a coal tar pitch containing green fluorescent bodies in a solvent having'a boiling point range substantially less than the lubricating oil, treatingthe solution containing the dissolved coal tar pitch with sulfuric acid in quantities sulficient to combine with the major portion of the carbonaceous content; separating the solvent containing the green fluorescent bodies from the acid reaction products, com mingling the solvent containing the green fluorescent bodies with a lubricating oil stock, separating by distillation the solvent from the lubricating oil and green fluorescent bodies, and finally clarifying and decolorizing to the required degree.

7, A process for the manufacture of lubrieating oil with a desired green fluorescence, comprising dissolving a'coal tar pitch containing green fluorescent bodies in a solvent hydrocarbon oil having a boiling point range substantially the, same as the lubricating'oil, treating the solution containing the dissolved coal tar pitch with sulfuric acid in quantities suflicient to combine with substantially all the black carbonaceous material contained therein, separating the solvent containing the green fluorescent bodies from the acid reaction products, and f... tlly commingling the solvent containing the green fluorescent 8. A process for the manufacture of lubri eating oil with a desired green fluorescence, comprising dissolving a coal tar pitch containing green fluorescent bodies in a lubricating oil, treating the lubricating oil containing thedissolved coal tar pitch with sulfuric acid in quantities suflicient to combine substantially with all the black carbonaceous content, separating the lubricating oil containing the green fluorescent bodies from. the acid reaction products, commingling the lubricating oil containing t 1e green fluorescent bodies with other lubricating oil, which is lacking in green fluorescent bodies, and a decolorizing clay at temperatures substan-' solved high flash coal tar distillate and green fluorescent bodies, and then separating the clarified and decolorized lubricating oil containing the hydrocarbon oil, high flash coal tar distillate and green fluorescent bodies from the decolorizing clay and adsorbed constituents.

10. A process for the manufacture of lubrieating oil with a desired green fluorescence, comprising dissolving a coal tar distillate containing green fluorescent bodies in a solvent having a boiling point range substantially less than the lubricating oil, treating the solution containing the dissolved coal tar distillate with sulfuric acid in quantities sufficient to combine with a major portion of the colored carbonaceous material; separating the solvent containing the green fluorescent bodies from the acid reaction products; commingling the solvent containing the green fluorescent bodies with the lubricating oil stock; separating by distillation the solvent from the lubricating oil and green fluorescent bodies and finally clarifying and decolorizing to the required degree.

11. A process for the manufacture of mbricating oil with a desired green fluorescence, comprising dissolving a coal tar distillate containing green fluorescent bodies in a solvent hydrocarbon oil having a boiling point range substantially the same as the lubricating oil, treating the se containing the dissolved coal tar distillate with sulfuric acid inquantities sulficient to combine with substantially all the colored carbonaceous material; separating the solvent contain lUL ing the green fluorescent bodies from the acid reaction products, and finally commingling the solvent containing the green fluorescent bodies with the lubricating oil. l 12. A process for the manufacture of lubricating oil with a desired green fluorescence, comprising dissolving a coal tar distillate containing green fluorescent bodies in a lubricating oil, treating the lubricating oil containing the dissolved coal tar distillate with sulfuric acid in quantities sufficient to combine substantially with all .the colored carbonaceous material; separating the lubricating oil containing the green fluorescent bodies from the acid reaction products, c0m mingling the lubricating oil containing the green fluorescent bodies with other lubricating oil, which is lacking in green fluorescent bodies, and a decolorizing clay at temperatures substantially not less than 230 F., and finally separating by filtration the combined lubricating oil containing the green fluorescent bodies from the decolorizing clay and adsorbed constituents. In testimony whereof we aifix our signatures.

JOHN C. BLACK. WIRT D. RIAL. JOHN R. McCONNELL. 

